CN201933200U - Oxidation resistant coating for guide flow cylinder - Google Patents
Oxidation resistant coating for guide flow cylinder Download PDFInfo
- Publication number
- CN201933200U CN201933200U CN201120005359XU CN201120005359U CN201933200U CN 201933200 U CN201933200 U CN 201933200U CN 201120005359X U CN201120005359X U CN 201120005359XU CN 201120005359 U CN201120005359 U CN 201120005359U CN 201933200 U CN201933200 U CN 201933200U
- Authority
- CN
- China
- Prior art keywords
- coating
- silicon carbide
- guide shell
- carbon
- oxidation resistant
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Lifetime
Links
Images
Abstract
The utility model discloses an oxidation resistant coating for a guide flow cylinder with simple technology and good inoxidability of the coating. The oxidation resistant coating comprises a substrate prepared by carbon/carbon composite material, and is characterized in that a transition layer (2) composed of a silicon carbide whisker in in-situ growth is arranged on the surface of the substrate. The guide flow cylinder substrate is processed conveniently; a layer of silicon carbide whiskers in in-situ growth is arranged on the guide flow cylinder substrate; the size and the number of cracks in the coating are reduced and decreased by using the connection between an pull-out bridge for the silicon carbide whisker and a crack steering mechanism, so that the oxidation resistance and the thermal shock stability of the silicon carbide coating are greatly improved; and the whole preparation process is continuously finished through chemical vapor deposition, so that the preparation process of the coating is greatly simplified, and the combination property of the guide flow cylinder is improved.
Description
Technical field
The utility model relates to a kind of thermal field of single crystal furnace part guide shell, specifically a kind of guide shell oxidation resistant coating, and particularly relating to a kind of guide shell is the surface oxidation-resistant coating of matrix by carbon/carbon compound material.
Background technology
Guide shell is the crucial thermal field component that monocrystalline silicon draw machines must be used, and is mainly used in the thermograde and the guiding argon gas stream of control thermal field, and this will ask the heat-insulating property of guide shell own to get well, and have certain anti-airflow scouring ability.At present single-crystal furnace guide shell is generally made by graphite piece and the combination of carbon felt, promptly goes out inner core and urceolus with machining graphite, and the carbon felt is clipped in the middle of inner core and the urceolus, by fastening piece the three is combined again.The shortcoming of this guide shell is: (1) causes guide shell shorter work-ing life because graphite intensity is low; (2), cause heat-preservation cylinder processing to use comparatively loaded down with trivial details because the good heat conductivity of graphite in order to improve heat-insulating property, must add one deck carbon felt between graphite inner core and urceolus; (3) large size guide shell shaping difficulty, consumptive material is more.Therefore, in recent years, the whole guide shell of many silicon single-crystal manufacturer's employing carbon-fibre composites replaces graphite carbon felt combination guide shell to carry out the drawing of silicon single crystal rod, makes the problems referred to above obtain solving preferably.
But, because guide shell is to use under the high temperature silicon steam condition, molten silicon under the high temperature has extremely strong reactive behavior, generate oxidizing substance such as SiO with quartz crucible reaction and volatilize from bath surface, oxidizing substances such as the SiO that volatilizes are centered around the outside surface of guide shell, and along with the prolongation of time, the guide shell outside surface is corroded gradually and forms the hole, hole, influence its result of use, reduced work-ing life.Therefore, in order to improve the resistance to corrosion of guide shell under the high temperature silicon steam condition, further improving its work-ing life, is best choice in guide shell surface preparation coating, and the erosion-resisting characteristic of coating will prolong the work-ing life of guide shell.
For improving the anti-oxidant and anti-thermal shock ability of guide shell, therefore, need be in carbon/carbon compound material guide shell surface preparation oxidation resistant coating.At present, method commonly used is to adopt the chemical vapor deposition (CVD) legal system to be equipped with coating, and the characteristics that the CVD method prepares oxidation resistant coating are: the coating densification is smooth, purity is high, and can realize the design to coating structure, pattern, composition and thickness.Therefore, the CVD coating technology is widely used in semi-conductor, metallurgy industry etc. with high temperature, highly purified various heat structure parts surface coatings, and is wherein extensive with the SiC coatings applications.It is bigger that SiC has unreactiveness, the excellent high-temperature mechanical property, and thermal shock resistance and resistance of oxidation, high fusing point, and also the reaction of SiC high temperature oxidation can generate continuous, even, fine and close SiO
2The oxidation protection film is so SiC coating and SiC compound coating are the preferred material of carbon/carbon compound material oxidation resistant coating.But the oxidation-protective effect of SiC coating that develops at present and SiC compound coating is far away from theoretical value, and its major cause is well not resolve the structure problem of coating.As application number is 200910310354.5, publication No. is CN101717992A, denomination of invention is that a kind of CZ silicon crystal growth oven carbon one carbon composite guide shell and preparation method thereof discloses and a kind ofly guide shell is carried out surface oxidation-resistant anti-impact erosion resisting coating handles, and the guide shell surface is provided with coat of silicon carbide.Because carbon/carbon composite material base body and SiC thermal expansivity do not match, the prepared SiC coating and the associativity of carbon/carbon composite material base body are relatively poor, come off easily, ftracture, and do not have well to solve the problem of the anti-airflow scouring ability of guide shell.
Simultaneously, adopt the whole preparation of carbon/carbon compound material guide shell, when precast body is made, its flange be formed with certain degree of difficulty, and because of the deformation factor in the subsequent thermal processing process that will consider whole guide shell precast body, often do the flange of whole guide shell precast body thicker, increased difficulty of processing, consumptive material is also more.
Summary of the invention
The purpose of this utility model provides a kind of guide shell oxidation resistant coating of coating good in oxidation resistance, particularly provide a kind of on the guide shell matrix growth in situ one deck silicon carbide whisker transition layer be oxidation resistant coating.
The utility model is to adopt following technical scheme to realize its goal of the invention, a kind of guide shell oxidation resistant coating, and it comprises that the surface of matrix is provided with the transition layer of being made up of the silicon carbide whisker of growth in situ by the matrix of carbon/carbon compound material preparation.
The utility model is further to improve anti-oxidation of coating, and transition layer is provided with the top layer of being made up of compact silicon carbide.
The utility model is easy to process, and described matrix comprises cylindrical shell, flange, and cylindrical shell, flange connect by web member.
A kind of in the screw made with carbon/carbon compound material or bolt or double-screw bolt or the pin of web member described in the utility model.
Owing to adopt technique scheme, the utility model has been realized goal of the invention preferably, the guide shell matrix is easy to process, growth in situ one deck silicon carbide whisker on the guide shell matrix, the silicon carbide skin of refabrication densification, thereby between the silicon carbide top layer of matrix and densification, form the SiCw transition layer, its thermal expansivity is between matrix and silicon carbide, can effectively reduce because the thermal stresses that thermal expansivity does not match and produces, simultaneously, utilize extract bridging and the crackle of silicon carbide whisker to turn to mechanism to reduce crack size and quantity in the coating, help increasing substantially the antioxidant property and the thermal shock resistance of coat of silicon carbide, and whole process of preparation can finish continuously by chemical vapour deposition, simplified the preparation process of coating greatly, improved guide shell over-all properties.
Description of drawings
Fig. 1 is the structural representation of the utility model guide shell;
Fig. 2 is that the utility model is at the structural representation of guide shell matrix surface preparation by the transition layer of being made up of silicon carbide whisker;
Fig. 3 is the surface scan electromicroscopic photograph of the utility model at the silicon carbide whisker of guide shell matrix surface growth in situ;
Fig. 4 is the X-Ray diffracting spectrum of the utility model at the silicon carbide whisker of guide shell matrix surface growth in situ;
Fig. 5 is the cross section stereoscan photograph of the utility model at the silicon carbide whisker of guide shell matrix surface growth in situ;
Fig. 6 is the A place enlarged diagram of Fig. 1;
Fig. 7 is the utility model when the preparation of guide shell matrix surface has transition layer and top layer, the surface scan electromicroscopic photograph on top layer;
Fig. 8 is the utility model embodiment 6(curve II), embodiment 8(curve III), embodiment 2(curve IV), embodiment 10(curve V) with SiC coating sample (curve I) isothermal oxidation weight loss curve in 1100 ℃ of air of traditional chemical vapour deposition process preparation;
Fig. 9 is the utility model embodiment 6(curve II), embodiment 8(curve III), embodiment 2(curve IV), embodiment 10(curve V) with SiC coating sample (curve I) air of traditional chemical vapour deposition process preparation in 15 1100 ℃ * 3min of experience ← → the oxidation weight loss curve of room temperature * 3min thermal cycling.
Embodiment
The utility model is described in further detail below in conjunction with drawings and Examples.
Embodiment 1:
As seen from Figure 1, Figure 2, a kind of guide shell oxidation resistant coating, it comprises that the surface of matrix is provided with the transition layer of being made up of the silicon carbide whisker of growth in situ 2 by the matrix of carbon/carbon compound material preparation.
A kind of preparation method of the oxidation resistant coating of guide shell as mentioned above, it may further comprise the steps:
⑴ get the raw materials ready: with the polishing of guide shell matrix, polishing, dry for standby after the washes clean;
⑵ Preparation of Catalyst: the presoma alcohol solution of preparation catalyzer makes Ni in the solution
2+: Al
3+=(5～15): (1～3) (present embodiment is Ni
2+: Al
3+=5:1), 5%～20%(present embodiment that the alcoholic acid volume accounts for overall solution volume is 20%), add aqueous solution of urea, regulate making Ni
2+Concentration for (0.05～0.2) mol/L(present embodiment be 0.1mol/L), transfer in the reactor after stirring;
⑶ loading catalyst: it is 10 h that step ⑴ gained matrix is put into reactor solution normal pressure dipping 5h～12h(present embodiment), reacting 1h～3h(present embodiment in the oil bath with reactor immersion 95 ℃～120 ℃ (present embodiment is 110 ℃) then is 2h), after reactor is chilled to room temperature with cold water matrix 1 is therefrom taken out, the back of drying in the shade at normal temperatures is stand-by;
⑷ growth in situ silicon carbide whisker: step ⑶ gained matrix is put into chemical vapor deposition stove; be evacuated to 0.1kPa; feed argon gas; under argon shield, heat up; depositing temperature is 950 ℃～1250 ℃ (present embodiment is 1100 ℃); 10min～60min(present embodiment is 15min before arriving depositing temperature) close argon gas; feeding hydrogen reduces to catalyzer; hydrogen flowing quantity is that 100mL/min～300mL/min(present embodiment is 200mL/min); reach that to be incubated 10min～60min(present embodiment behind the depositing temperature be 15min); then with hydrogen as carrier gas and diluent gas; throughput ratio is 1:1; with Bubbling method trichloromethyl silane is introduced in the cvd furnace; the container bottle of splendid attire trichloromethyl silane places water bath with thermostatic control, and 18 ℃～25 ℃ of bath temperatures (present embodiment is 22 ℃), depositing time are that 1h～50h(present embodiment is 6h); pressure is normal pressure, prepares the transition layer of being made up of the silicon carbide whisker of growth in situ 2 at matrix surface.
Embodiment 2:
Present embodiment is convenient processing, and in step ⑴, described guide shell matrix comprises cylindrical shell 1, flange 4, and cylindrical shell 1, flange 4 connect by web member 5.A kind of in the screw made with carbon/carbon compound material or bolt or double-screw bolt or the pin of described web member 5, the pin of present embodiment for making with carbon/carbon compound material.
Surplus with embodiment 1.
As shown in Figure 3, the silicon carbide whisker of the utility model preparation is evenly distributed at the guide shell matrix surface.
As shown in Figure 4, the utility model is β-SiCw at the silicon carbide whisker of guide shell matrix surface growth in situ.
As shown in Figure 5, cross section stereoscan photograph explanation silicon carbide whisker transition layer 2 porous of guide shell matrix and fine and close gradually along the direction of carbon/carbon composite material base body, this explanation transition layer 2 is fine with matrix bond, simultaneously, transition layer 2 porous surfaces, when being provided with the top layer of forming by compact silicon carbide thereon again, help alleviating the thermal stresses of coating inside, avoid coating cracking and come off.
Embodiment 3:
As shown in Figure 6, the utility model is further to improve anti-oxidation of coating, is provided with the top layer of being made up of compact silicon carbide 3 on transition layer 2.
Its preparation technology is in step ⑷, and depositing time is 2h.
After step ⑷ is intact, diluent gas is changed into argon gas, carrier gas is a hydrogen, and the adjustment diluting gas flow is 2:1 with the carrier gas flux ratio, depositing temperature is 950 ℃～1250 ℃ (present embodiment is 1100 ℃), and depositing time is that 1h～50h(present embodiment is 4h), pressure is normal pressure.The top layer 3 that preparation is made up of compact silicon carbide on the transition layer of being made up of the growth in situ silicon carbide whisker 2.
As shown in Figure 7, compact silicon carbide top layer 3 densifications, smooth are attended by a small amount of little crackle, but do not have tangible hole, compact silicon carbide top layer 3 be describeds in the evenly formation of silicon carbide whisker transition layer 2 surfaces, good consistency are arranged between two-layer.
Surplus with embodiment 1.
Embodiment 4:
Present embodiment is convenient processing, and in step ⑴, described matrix comprises cylindrical shell 1, flange 4, and cylindrical shell 1, flange 4 connect by web member 5.A kind of in the screw made with carbon/carbon compound material or bolt or double-screw bolt or the pin of described web member 5, the pin of present embodiment for making with carbon/carbon compound material.
Surplus with embodiment 1, embodiment 3.
Embodiment 5:
In step ⑷, depositing time is 3h, and during preparation top layer 3, depositing time is 3h.
Surplus with embodiment 1, embodiment 3.
Embodiment 6:
Present embodiment is convenient processing, and in step ⑴, described matrix comprises cylindrical shell 1, flange 4, and cylindrical shell 1, flange 4 connect by web member 5.A kind of in the screw made with carbon/carbon compound material or bolt or double-screw bolt or the pin of described web member 5, the pin of present embodiment for making with carbon/carbon compound material.
In step ⑷, depositing time is 3h, and during preparation top layer 3, depositing time is 3h.
Surplus with embodiment 1, embodiment 3.
Embodiment 7:
In step ⑷, depositing time is 5h, and during preparation top layer 3, depositing time is 1h.
Surplus with embodiment 1, embodiment 3.
Embodiment 8:
Present embodiment is convenient processing, and in step ⑴, described matrix comprises cylindrical shell 1, flange 4, and cylindrical shell 1, flange 4 connect by web member 5.A kind of in the screw made with carbon/carbon compound material or bolt or double-screw bolt or the pin of described web member 5, the pin of present embodiment for making with carbon/carbon compound material.
In step ⑷, depositing time is 5h, and during preparation top layer 3, depositing time is 1h.
Surplus with embodiment 1, embodiment 3.
As shown in Figure 8, the resistance of oxidation of the SiC coating sample of traditional chemical vapour deposition process preparation is the poorest, and oxidation 10h rate of weight loss is 41.11% in 1100 ℃ of air, among Fig. 8 shown in the curve I.
Oxidation 10h rate of weight loss is respectively in 1100 ℃ of air of four embodiment coating samples of the utility model preparation: 8.87%(embodiment 4, shown in the curve II), 5.50%(embodiment 6, shown in the curve III), 2.07%(embodiment 2, shown in the curve IV) and 0.87%(embodiment 8, shown in the curve V), its average rate of weight loss is 4.33%.
As shown in Figure 9, the thermal shock resistance of the SiC coating sample of traditional chemical vapour deposition process preparation is the poorest, 1100 ℃ * 3min ← → 15 thermal cyclings of room temperature * 3min after rate of weight loss be 33.17%, among Fig. 9 shown in the curve I.
And four embodiment coating sample rate of weight loss of the utility model preparation are respectively: 11.09%(embodiment 4, shown in the curve II), 5.66%(embodiment 6, shown in the curve III), 0.51%(embodiment 2 is shown in the curve IV) and 0.22%(embodiment 8, shown in the curve V).
The SiC coating for preparing for the ease of the coating of relatively the utility model preparation and traditional chemical vapour deposition process is in the difference aspect antioxidant property and the thermal shock resistance, the depositing time of all embodiment floating coats of the utility model is identical, and promptly the depositing time of the depositing time of growth in situ silicon carbide whisker or growth in situ silicon carbide whisker and fine and close SiC coating depositing time sum are 6h.
Silicon carbide whisker is that a kind of diameter is an extremely micron-sized single crystal fibre of nano level, has good characteristics such as high strength, high rigidity, high elastic coefficient and density are low, corrosion-resistant, chemical property stable, oxidation-resistance property is strong.The utility model is by in surface preparation growth in situ SiCw coating that is prepared guide shell by carbon/carbon compound material and the toughness reinforcing SiCw-SiC coating of SiCw, the oxidation-resistance of coating and thermal shock resistance increase substantially than the SiC coating of traditional method preparation, and realized the coating preparation of serialization under the normal pressure, adopt plurality of raw materials, several different methods to prepare the technology of coating with respect to other, simplified the preparation process of coating greatly, improved greatly guide shell over-all properties, help promoting the use of of coating.
Claims (4)
1. guide shell oxidation resistant coating, it comprises by the matrix of carbon/carbon compound material preparation, it is characterized in that the surface of matrix is provided with the transition layer of being made up of the silicon carbide whisker of growth in situ (2).
2. guide shell oxidation resistant coating according to claim 1 is characterized in that transition layer (2) is provided with the top layer of being made up of compact silicon carbide (3).
3. guide shell oxidation resistant coating according to claim 1 and 2 is characterized in that described matrix comprises cylindrical shell (1), flange (4), and cylindrical shell (1), flange (4) connect by web member (5).
4. guide shell oxidation resistant coating according to claim 3 is characterized in that a kind of in the screw made with carbon/carbon compound material or bolt or double-screw bolt or the pin of described web member (5).
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201120005359XU CN201933200U (en) | 2011-01-10 | 2011-01-10 | Oxidation resistant coating for guide flow cylinder |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201120005359XU CN201933200U (en) | 2011-01-10 | 2011-01-10 | Oxidation resistant coating for guide flow cylinder |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN201933200U true CN201933200U (en) | 2011-08-17 |
Family
ID=44444733
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201120005359XU Expired - Lifetime CN201933200U (en) | 2011-01-10 | 2011-01-10 | Oxidation resistant coating for guide flow cylinder |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN201933200U (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103570378A (en) * | 2012-08-01 | 2014-02-12 | 苏州宏久航空防热材料科技有限公司 | Method for direct deposition of silicon carbide (SiC) coating on carbon material surface in graphite heat-generating body heating furnace |
-
2011
- 2011-01-10 CN CN201120005359XU patent/CN201933200U/en not_active Expired - Lifetime
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103570378A (en) * | 2012-08-01 | 2014-02-12 | 苏州宏久航空防热材料科技有限公司 | Method for direct deposition of silicon carbide (SiC) coating on carbon material surface in graphite heat-generating body heating furnace |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN102167623B (en) | Carbon material oxidation resistant coating and preparation method thereof | |
| WO2021027469A1 (en) | Sicf/sic composite material burner inner liner and automatic preparation method therefor | |
| Fan et al. | Preparation of nickel coating on ZTA particles by electroless plating | |
| CN107540400A (en) | A kind of SiC with compound interfacef/ SiC ceramic based composites | |
| CN102021648B (en) | Guide cylinder antioxidation coating and preparation method thereof | |
| CN109553430A (en) | A kind of SiC with compound interfacef/ SiC ceramic based composites and preparation method thereof | |
| CN101863665B (en) | Method for preparing self-healing anti-oxidation functional fiber reinforced ceramic matrix composite material | |
| CN102295474B (en) | Preparation method of SiC-TaC coating/matrix collaborative modified C/C composite material | |
| CN102731119B (en) | Crucible using carbon/carbon/silicon carbide composite material and preparation method thereof | |
| CN113845367B (en) | Preparation method of high-temperature oxidation-resistant carbon fiber toughened zirconia ceramic material and high-temperature oxidation-resistant carbon fiber toughened zirconia ceramic material | |
| CN102718539B (en) | Carbon/carbon/silicon carbide composite material thermal-insulation barrel and preparation method | |
| CN109400169A (en) | SiC with SiC coatingfPreparation method of/SiC composite material | |
| CN105481477B (en) | A kind of preparation method of graphite/SiC ceramic matrix composite material | |
| CN102123527B (en) | Application and preparation method of carbon material heating body | |
| CN201915039U (en) | Carbon material anti-oxidation coating | |
| CN107630184B (en) | A method of niobium silicide coating is prepared in niobium or niobium alloy surface | |
| CN201915043U (en) | Heating element made of carbon materials | |
| CN104150938B (en) | The preparation method of one dimension hafnium carbide HfC material modification carbon/carbon composite | |
| CN201933200U (en) | Oxidation resistant coating for guide flow cylinder | |
| CN110042468A (en) | A kind of preparation method of micrometer silicon carbide zirconium whisker | |
| CN102531606A (en) | Low-temperature manufacturing method of high-strength and toughness silicon carbide ceramics | |
| Xu et al. | High-quality SiC-HfC coating with interpenetrating structure based on a two-step low temperature molten salt method | |
| CN105642877A (en) | High-strength composite submersed nozzle combined with silicon carbide crystal whiskers and manufacturing method | |
| CN110042653A (en) | A kind of surface has the carbon fiber and preparation method thereof of multiple dimensioned SiC-SiOC ceramic coating | |
| CN106747453B (en) | High-temperature cracking treatment method for SiC composite fiber winding cladding |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| C56 | Change in the name or address of the patentee | ||
| CP01 | Change in the name or title of a patent holder |
Address after: 413000 Hunan province Yiyang Yingbin Road No. 2 Patentee after: Hunan gold carbon Limited by Share Ltd Address before: 413000 Hunan province Yiyang Yingbin Road No. 2 Patentee before: Hunan KBCarbon Composite Science and Technology Co., Ltd. |
|
| CX01 | Expiry of patent term |
Granted publication date: 20110817 |
|
| CX01 | Expiry of patent term |